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A Rapid Separation and Highly Determination of Paraben Species by Ultra-Performance Liquid Chromatography —Electrochemical Detection

机译:通过超高效液相色谱 - 电化学检测快速分离和高度测定羟基甲型

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In this study, a new technique was developed using rapid ultra-performance liquid chromatography (UPLC)-based separation coupled with electrochemical detection by a boron-doped diamond (BDD) electrode for the detection and quantification of three commonly used parabens (methylparaben (MP), ethylparaben (EP) and propylparaben (PP)). We aimed to reduce the analysis time by using UPLC coupled with a short reverse phase C 18 monolithic column (25 mm×4.6 mm). Operating the monolithic column at low back-pressure resulted in high flow rates. A mobile phaseconsisting of a 25:75 (v/v) ratio of acetonitrile:0.05 Mphosphate buffer (pH 5) at a flow rate of 2.5 mL·min?1 was used to perform the separation. The amperometric detection with the BDD electrode was found to be optimal and reliably reproducible at a detection potential of 1.5 V vs. Ag/AgCl. Under these conditions, the separation of the three targetanalytes (MP, EP and PP) was achieved in 2 min and was linear within a sample concentration range of 0.1 to 50.0 mg·L?1 (r2 values of 0.9970, 0.9994 and 0.9994 for MP, EP and PP, respectively). This method was successfully applied to determine the concentrations of each parabeninsix real samples with therecoveries ranging from of 80.3% - 98.9% for all three parabensfrom samples spiked at 12, 22 and 32 mg·L?1. Therefore, the proposed method can be used as an alternative rapid and selective method for the determination of paraben levels in real samples.
机译:在该研究中,使用快速超级性能液相色谱(UPLC)分离开发了一种新的技术,其通过硼掺杂的金刚石(BDD)电极进行电化学检测,用于检测和定量三种常用的羟基苯甲酸盐(甲基汤根(MP) ),乙基羟基苯(EP)和丙基羟基苯(PP))。我们旨在通过使用带有短反向相C 18单片柱(25mm×4.6mm)的UPLC耦合来减少分析时间。在低压压力下操作整体柱导致流量高。 25:75(v / v)比率的乙腈:0.05米米磷酸盐缓冲液(pH5)的流动阶段的比例用于2.5ml·min·1的流速进行分离。在1.5V与Ag / AgCl的检测电位,发现具有BDD电极的安培测量检测是最佳的并且可靠地再现。在这些条件下,在2分钟内实现三个靶标分析(MP,EP和PP)的分离,并在0.1至50.0mg·L·1(R2值为0.9970,20.994和0.9994的样品浓度范围内的线性,EP和PP)分别)。该方法被成功地应用于确定每个羟基茚单因的真实样品的浓度,其在12,22和32mg·L≥1中掺入的所有三种羟基烷基的80.3×%-98.9 %。因此,所提出的方法可以用作确定真实样品中羟基甲醚的替代快速和选择性方法。

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